Sodium Hydroxide → HCID 57285652, 화합물

HRID 648660노트

반응식

HRID 648660 반응식
[N:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[CH:13]([CH:17]([C:29]([NH2:31])=[O:30])[C:18]2[CH:28]=[CH:27][C:21]([C:22](OCC)=[O:23])=[CH:20][CH:19]=2)[CH2:14][CH2:15][CH3:16])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+]>O1CCCC1>[N:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[CH:13]([CH:17]([C:29]([NH2:31])=[O:30])[C:18]2[CH:19]=[CH:20][C:21]([CH2:22][OH:23])=[CH:27][CH:28]=2)[CH2:14][CH2:15][CH3:16])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 20145118HCID 20145118, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 57285652HCID 57285652, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 5.0 gm (11.83 m mol) of ethyl 4-[(1-(2-piperidino-phenyl)-1-butyl)-aminocarbonylmethyl]-benzoate in 75 ml of absolute tetrahydrofuran was added dropwise, at an internal temperature of 0° C., to a stirred suspension of 0.68 gm (17.95 m mol) of lithium aluminium hydride in 25 ml of absolute tetrahydrofuran. The mixture was stirred for 20 hours at ambient temperature and then cooled to 0° C., and 4N sodium hydroxide solution was slowly added dropwise thereto until a filterable precipitate formed. The mixture was filtered, and the precipitate was decocted several times with ether. The combined organic solutions were concentrated by evaporation in vacuo. The evaporation residue was distributed between water and ether. The ether phase was dried, filtered, and concentrated by evaporation in vacuo. The evaporation residue was purified by column chromatography on silica gel [toluene/acetone (5:1)].

후처리

  1. temperaturecooled to 0° C.
  2. customuntil a filterable precipitate formed
  3. filtrationThe mixture was filtered
  4. concentrationThe combined organic solutions were concentrated by evaporation in vacuo
  5. dry with materialThe ether phase was dried
  6. filtrationfiltered
  7. concentrationconcentrated by evaporation in vacuo
  8. customThe evaporation residue was purified by column chromatography on silica gel [toluene/acetone (5:1)]

출처 및 근거

ORD 기록
ord-d4e62fc588d44899a207ba65363bfa9e
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04735959

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